Draft Indian Standard TOBACCO AND TOBACCO ...2786-2913)_18022015.pdf1 For BIS Use Only DRAFT FOR COMMENTS ONLY Doc: No. FAD 04(2786)C Draft Indian Standard TOBACCO AND TOBACCO PRODUCTS

1

For BIS Use Only

DRAFT FOR COMMENTS ONLY Doc: No. FAD 04(2786)C

Draft Indian Standard

TOBACCO AND TOBACCO PRODUCTS

DETERMINATION OF REDUCING AND TOTAL SUGARS ICS No. 65.160

Not to be reproduced or used as

STANDARD without permission of BIS

Last date for comments: April 20, 2015

Tobacco and Tobacco Products Sectional Committee, FAD 4

FOREWORD

(Adoption clause would be added later)

The chemical properties of leaf tobacco are influenced by agricultural practices, soil type and nutrients, weather

conditions, stalk position and curing procedures. A change in any of these factors can markedly alter the

chemical composition of tobacco leaf and thus affect the quality of tobacco products.

The total and reducing sugar contents of tobacco are important indicators of the quality of tobacco raw materials

and finished tobacco products. This standard will help in getting uniform and reproducible results while

determining the total and reducing sugar contents in tobacco and tobacco products and thereby a consistent

quality product.

In reporting the result of a test or analysis made in accordance with this standard, is to be rounded off, it shall be

done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)'. The number of

significant places retained in the rounded off value should be the same as that of the specified value in this

standard.

1 Scope

This standard specifies a method for the determination of reducing and total sugars in tobacco and tobacco

products by iodometric titration method.

2 REFERENCES

The standards given below contain provisions which, through reference in this text, constitute provisions of this

standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and

parties to agreements based on this standard are encouraged to investigate the possibility of applying the most

recent editions of these standards.

IS No. Title

5643 : 1999 Tobacco and tobacco products Method of test for tobacco (second revision)

3 TERMINOLOGY

For the purpose of this standard, the following definitions shall apply.

3.1 Reducing Sugars Sugar that, in its native form, can reduce the alkaline copper oxide into cuprous oxide,

is classified as reducing sugar. The ability of an aqueous extract of tobacco to cause this reduction is indicative

of the presence of reducing sugar and can be quantified by the method prescribed in this standard.

3.2 Non Reducing Sugars Water soluble carbohydrates, which do not possess the reducing property, but

acquires this property after acid hydrolysis. The difference in the sugar contents before and after hydrolysis is a

measure of non-reducing sugar content in tobacco.

2

3.3 Total Sugars The total of water-soluble reducing and non-reducing sugars is known as total sugars,

which are determined after acid hydrolysis according to the procedure described in this standard.

4 QUALITY OF REAGENTS

Unless specified otherwise, pure chemicals shall be employed in tests and distilled water shall be used where the

use of water as reagent is intended.

NOTE — 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the test results.

5 APPARATUS

Usual laboratory apparatus and in particular the following:

5.1 Fast Boiling Water Bath

5.2 Hot Plate or Heating Mantle

5.3 Whatman Filter Paper No. 40

5.4 Laboratory Mill, fitted with 1 mm sieve.

5.5 Timer

6 REAGENTS

6.1 Lead acetate, (CH3COO)2Pb.3H2O

6.2 Shaffer-Somogyi Carbonate Reagents

a) Sodium Carbonate, Na2CO3, Anhydrous

b) Potassium Sodium Tartarate (Rochelle Salt), KNaC4H4O6.4H2O

c) Copper Sulphate, CuSO4.5H2O, 10 percent solution Dissolve 7.5 g in 75 ml of distilled water.

d) Sodium Bicarbonate, Anhydrous, NaHCO3

e) Potassium iodate solution Dissolve 3.567 g of potassium iodate in 1 litre of distilled water.

f) Potassium Iodide

6.2.1 Preparation of Shaffer-Somogyi Reagent Dissolve 25 g of anhydrous sodium carbonate [6.2 (a)] and

25 g of Rochelle salt [6.2 (b)] in 500 ml of distilled water in 1 litre volumetric flask. Add with stirring 75 ml of

the copper sulphate solution [6.2 (c)] slowly by a pipette well below the surface of the liquid. Add 20 g sodium

bicarbonate [6.2 (d)], dissolve by stirring, then add 5 g of Potassium iodide [6.2 (f)]. When all the solids are

dissolved, add 200 ml of potassium iodate solution [6.2 (e)]. Make up the volume. Mix thoroughly and allow the

reagent to stand for two days and filter before use. The reagent is stable for one year if stored in an amber

coloured bottle.

6.3 Potassium Iodate Solution, 0.1 N.

6.4 Sodium Thiosulphate (Na2S2O3.5H2O) Solution, 0.1 N Dissolve 24.82 g of sodium thiosulphate and

0.2 g of sodium carbonate in 200 ml of distilled water and dilute to one litre.

6.4.1 Standardization Standardize the sodium thiosulphate solution (see 6.4) against 0.1 N potassium iodate

solution (see 6.3). For titration, take 25 ml of 0.1 N potassium iodate solution in a 250 ml conical flask, add

3 g of potassium iodide and 10 ml of 1 N sulphuric acid. Titrate against 0.1 N sodium thiosulphate until pale

yellow colour. Add approximately 65 ml of water and add 2 ml of starch indicator solution (see 6.6) and

continue titration till dark blue colour changes to colourless.

6.5 Sodium Thiosulphate Solution, 0.005N Prepare 0.005 N solution by diluting 25 ml of 0.1 N sodium

thiosulphate solution into 500 ml with water. The solution is unstable and hence should be discarded after

4 hours.

6.6 Starch Indicator Solution Disperse 1 g soluble starch in 20 ml water and pour into about 80 ml boiling

water. Boil for one minute and cool. Prepare a fresh starch solution daily.

6.7 Sodium Hydroxide Solution, 0.5 N.

3

6.8 Sulphuric Acid Solution, 2 N.

6.9 Hydrochloric Acid, 0.5 N.

6.10 Potassium Iodide Solution, 2.5 percent Weigh 2.5 g in 100 ml volumetric flask and dilute to volume

with distilled water.

6.11 Potassium oxalate

7 PRINCIPLE

An aqueous extract of the tobacco sample is prepared and the reducing sugars (as glucose) is determined by

Shaffer-Somogyi method. Cuprous oxide produced by the reaction of a reducing sugar with the Somogyi

reagent is reacted with potassium iodate in the presence of sulphuric acid. Excess potassium iodate is

determined by adding potassium iodide and titrating the liberated iodine with sodium thiosulphate solution using

starch as an indicator. The non-reducing sugars are hydrolysed with dilute hydrochloric acid and the total

reducing sugars (as glucose) is determined as above.

8 PROCEDURE

8.1 Preparation of Sample

Prepare the tobacco sample for analysis by grinding (the sample should totally pass through 1 mm sieve) and

determine the moisture content. Ideally moisture content shall be less than 15 percent for grinding. If the

tobacco is wet for grinding, it may be air dried.

8.2 Test Portion

Determine the oven moisture content of the ground sample by the method as prescribed in IS 5643.Transfer

about 1 g of ground sample, weighed to the nearest 0.01 g, to a 250 ml Erlenmeyer flask.

8.3 Extraction

Add exactly 100 ml of distilled water to the flask (see 8.2) and shake for 1 hour on a flask shaker and filter

through Whatman no. 40 filter paper. Add 0.5 g of lead acetate to the filtrate, shake well and allow to stand for

30 minutes.

8.4 Removal of Interfering Substances and Deleading

Filter the solution through a Whatman no. 40 filter paper into a dry 250 ml conical flask containing

1g potassium oxalate. Shake well and allow to stand for 30 minutes. Filter the solution through Whatman no. 40

filter paper into a dry 100 ml conical flask.

8.5 Preparation for Total Sugars Hydrolysis of Total Sugars

Pipette 10 ml of solution from 8.4 into a 50 ml conical flask, add 5 ml of 0.5 N hydrochloric acid and boil on hot

plate/heating mantle for 3-5 minutes. Cool to room temperature and add 5 ml of 0.5 N sodium hydroxide

solution. Transfer quantitatively to 50 ml volumetric flask and dilute to volume. Mix thoroughly.

8.6 Preparation for Reducing Sugars

Pipette 10 ml of the filtrate (8.4) into a 50 ml volumetric flask, Make up the volume.

9 DETERMINATION OF SUGAR

9.1 Pipette 5 ml aliquot from 8.6 (for reducing sugars) and 5 ml aliquot from 8.5 (for total sugars) into separate

100 ml conical flasks, add accurately 5 ml of the Shaffer Somogyi reagent to each flask and mix thoroughly.

Add anti-bumping granules and cover flasks with a glass bulb or funnel. Heat for exactly 15 minutes by

immersing in the boiling water bath. Ensure that the water level in the bath is above the reaction mixture.

Remove the flasks from the water bath, cool in cold water (20-25C) and add 2 ml of 2.5 percent KI solution by

4

running it from a pipette down the walls of the flask without stirring or agitation, add 3.0 ml of 2 N sulphuric

acid and mix thoroughly. Titrate the liberated iodine with 0.005 N thiosulphate solution till the solution becomes

pale yellow. Add 100 µl starch indicator solution and complete titration. The end point is blue to colourless.

9.2 Carry out 3 blank determinations using 5 ml of water in place of sample extract 9.1.

9.3 Subtract titre values of test solution from that of blank, and calculate the amount of glucose corresponding to

the titre difference from the formula.

10 CALCULATIONS

10.1 Calculate sugars (as glucose), percent by dry mass from the following formula:

Sugars (as glucose), percent by dry mass = G x V1 x V2 x 100 x 100

W x 1000 x V3 x V4 (100 - M)

where,

G = glucose in mg (see Table 1);

W = weight of sample in g;

M = percent moisture content;

V1 = volume of original sample extract (100 ml);

V2 = volume of diluted sample extract (50 ml);

V3 = volume of original sample extract used for dilution (10 ml); and

V4 = volume of sample used for titration (5 ml).

10.2 In case the titre values exceeds 17.9 ml, the following formula may be used for calculating mg glucose

Glucose, mg = 0.112 x (ml of 0.005 N sodium thiosulphate) + 0.04

ml of 0.005 N Sodium Thiosulphate = (Blank titre value – Sample titre value)

11 REPORTING

The report will carry the following:

a) Full identity of the sample;

b) Date of test;

c) Moisture content, percent of sample as received;

d) Reducing sugar content, percent on dry basis;

e) Total sugar content, percent on dry basis; and

f) Non-reducing sugar, percent on dry basis.

5

Table 1 Milligrams of Glucose Corresponding to the Difference between the Titration Values for the

Blank and the Unknown

(Clause 10.1)

0.005 N

Na2S2O3

(ml)

Milligram of Glucose Corresponding to Titration Difference of

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

(1) (2) (3) (4) (5) (6) (7) (8) (9) (10) (11)

0 0.05 0.06 0.08 0.09 0.10 0.11 0.13 0.14

1 0.15 0.16 0.17 0.19 0.20 0.21 0.22 0.21 0.24 0.35

2 0.27 0.28 0.29 0.30 0.31 0.32 0.33 0.35 0.36 0.37

3 0.38 0.39 0.41 0.41 0.42 0.43 0.45 0.46 0.47 0.48

4 0.49 0.50 0.53 0.54 0.54 0.55 0.56 0.57 0.58 0.59

5 0.60 0.61 0.64 0.65 0.65 0.66 0.67 0.68 0.69 0.70

6 0.72 0.73 0.74 0.75 0.76 0.77 0.78 0.79 0.80 0.82

7 0.83 0.84 0.85 0.86 0.87 0.88 0.89 0.90 0.91 0.83

8 0.94 0.95 0.96 0.97 0.98 0.99 1.00 1.01 1.02 1.04

9 1.05 1.06 1.07 1.08 1.09 1.10 1.11 1.12 1.13 1.15

10 1.16 1.17 1.18 1.19 1.20 1.21 1.22 1.23 1.24 1.26

11 1.27 1.28 1.29 1.30 1.32 1.33 1.34 1.35 1.36 1.37

12 1.38 1.39 1.40 1.42 1.43 1.44 1.45 1.46 1.47 1.48

13 1.49 1.50 1.52 1.53 1.54 1.55 1.56 1.57 1.58 1.59

14 1.60 1.61 1.63 1.64 1.65 1.66 1.67 1.68 1.69 1.70

15 1.71 1.72 1.74 1.75 1.76 1.77 1.78 1.79 1.80 1.81

16 1.82 1.83 1.85 1.86 1.87 1.88 1.89 1.90 1.91 1.92

17 1.93 1.94 1.95 1.96 1.97 1.98 1.99 2.01 2.02 2.03

1

For BIS Use Only



CIGARS AND CHEROOTS SPECIFICATION

PART 1 CIGARS

(Third Revision of IS 1769 Part 1) ICS No. 65.160





FOREWORD


Different types of cigars are manufactured in the country using tobaccos specifically grown and specially

processed for use in cigars. Cigars are also now being imported into the country. Thus, the range of cigars

available in the country is now much wider necessitating a thorough revision of the standard.

This standard was originally published in 1961 and subsequently revised in 1973 and 1994. This revision has

been undertaken to update the requirements of cigars on the basis of current industrial and trade practices,

advances in analytical science, and the prevailing statutory packaging and tobacco control rules and regulations.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,

observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with

IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in the

rounded off value should be the same as that of the specified value in this standard.

1 SCOPE

1.1 This standard prescribes requirements, methods of sampling and test for hand-made and machine-made

cigars.

1.2 It does not cover the requirements of flavour and aroma of cigars.

2 REFERENCES





IS No. Title

4905 : 1968 Methods for random sampling


10335 : 2007 Glossary of terms for tobacco and tobacco products (third revision)

16026 : 2012 Tobacco Determination of the content of total alkaloids as nicotine

/ISO 15152 : 2003 Continuous-flow analysis method

16132 : 2014 Tobacco and Tobacco Products Determination alkaloid content

/ISO 2881 : 1992 Spectrometric Method

16236 : 2014 Tobacco and tobacco products Determination of silicated residues

/ISO 2817 : 1999 insoluble in hydrochloric acid

2

3 DESCRIPTION

3.1 Cigar, a smoking article made entirely of tobacco, is composed of tightly rolled filler tobacco leaf, bound by

binder tobacco and wrapped in wrapper tobacco. Cigars are made by rolling with hands and also by rolling on

machines. In case of hand-made cigars, the three components - filler, binder and wrapper are all of natural

tobaccos, while in case of machine-made cigars, the binder and wrapper can be of homogenized tobacco leaf

(HTL, see 3.2.4) or natural leaf. Hand-made cigars are made from long filler and machine made cigars are made

from short filler.

The main cylindrical part of the cigar is called body, the mouth end of a cigar is called head, and the other end

which is lit, is called foot. Machine-made cigars shall be open at both ends unless a filter is attached at one end,

whereas hand-made cigar shall be open at one end and capped at the other end.

Cap is a circular piece of wrapper leaf glued to the head of a cigar for appearance as well as preventing the

wrapper from unravelling.

A band is a paper or foil ring loosely wrapped around a cigar, it can identify the brand/ make or be just

decorative.

3.2 Cigar tobaccos are of distinct variety yielding large leaves producing typical cigar aroma with good burning

quality and are grown in identified areas having required soil and climatic conditions.

For lighter leaf and thinner veins, tobacco is grown in the shade while tobacco grown in the sun yields darker,

thick veined and oily leaf. Shade-grown tobacco leaves are less oily as compared to sun-grown tobacco. Cigar

tobaccos are first air-cured and then fermented to generate the desired aroma, taste, texture and feel which are

important considerations for cigar products. Three different kinds of tobacco leaves with distinct characteristics

are used in making cigars that is filler, binder and wrapper. Different types of Indian tobaccos are described in

IS 10335.

3.2.1 Filler leaf, as the name suggests, fills up the body of the cigar to give it shape and size. It shall be properly

bunched to allow even burn and smoke to be drawn. It shall consist of fermented air-cured cigar tobaccos, a

blend of different varieties of filler tobaccos is usually used to impart the characteristic aroma and flavour.

3.2.2 Binder leaf, as the name suggests, binds the rolled filler tobacco and holds it together and in shape.

HTL may also be used as a binder. This assembly of filler bound by a binder is called bunch.

3.2.3 Wrapper leaf, as the name suggests, wraps around the bunch of filler tobacco and binder and holds the

whole cigar together. Wrapper, being the outermost visible component, is the most important component of a

cigar, as it gives the cigar its aesthetic appeal, texture and to a large extent its flavour and aroma. The leaf is

specially cured and fermented to develop its colour and aroma. The leaf is handled with utmost care throughout

its cycle from being picked from the plant till used on a cigar, to ensure that it remains free from damage and

blemish.

Wrapper leaf is the most expensive component of a hand-made cigar. The colour of the wrapper is linked to its

flavour and character, hence the colour is often used to describe a cigar as a whole. Traditionally, all cigars in a

packet should have the same colour.

3.2.4 Homogenized Tobacco Leaf (HTL) is tobacco leaf which has been macerated into a fine slurry and

converted into tobacco sheet, HTL may or may not contain non-tobacco material depending upon its end use as

different grades are used as binder and wrapper. HTL shall have sufficient mechanical strength to run

continuously on a cigar making machine.

3.2.5 Plume (also called bloom) is a desirable white crystalline deposit which occurs on the surface of a cigar

indicative of good aging of a cigar in optimal conditions of storage (close to 21°C and 70 percent relative

humidity). The exact nature of the white deposit is not much understood but is considered to be due to the

essential oils which exude through the wrapper and get deposited on the surface. Plume should not be mistaken

for mould. While plume is a desirable white solid spots spread on the cigar and can be easily wiped clean or

brushed away clean. Mould is woolly moist mass, cannot be brushed away and has a strong musty undesirable

smell.

3

3.3 REQUIREMENTS

3.3.1 Size

The size of cigars shall be as agreed between the buyer and vendor. The size of a cigar is measured by two

dimensions, its length and its diameter. The length can be measured by using a metric scale with an accuracy of

0.5 mm and is expressed in mm. The length can also be measured and expressed in inches.

The diameter of a cigar is measured by a ring gauge sizer and expressed as ring gauge. The unit of ring gauge

when expressed in inches is sixty-fourth (1/64) of an inch. For example, a ring gauge of 32 would be half an

inch in diameter. The diameter can also be measured and expressed in mm.

3.3.2 Mean Mass of Cigars

The mass of cigars shall be as agreed between the buyer and vendor and can be determined using a routine

analytical balance having a resolution of 0.001 g.

3.4 Freedom from Tobacco Beetle Attack

Cigars shall be free from any tobacco beetle attack when examined by the method prescribed in Annex A.

3.5 The material shall also conform to the requirements specified in Table 1.

Table 1 Requirements for Cigar

(Clause 3.5)

Sl

No.

Characteristics Requirement Method of Test,

Ref to

(1) (2) (3) (4)

i) Oven moisture content, percent by mass, Max 16.0 6 of IS 5643

ii) Total alkaloids as nicotine (on dry basis), percent by

mass, Max

3.5 8 of IS 5643 or

IS 16132 or IS 16026

iii) Total ash (on dry basis), percent by mass, Max 25.0 10 of IS 5643

iv) Silicated residues insoluble in hydrochloric acid (on

dry basis), percent by mass, Max

5.0 IS 16236

4 SORTING

After manufacture, cigars shall be graded according to the colour of the wrapper. Cigars of uniform colour will

be packed in one packet.

5 PACKING

Cigars shall be packed in retail containers of wooden, tin or cardboard or as agreed to between the purchaser and

the vendor. Individual cigars could be wrapped in additional suitable wrapping before packing in retail package.

Each cigar shall bear the trade-mark or brand name or the manufacturer’s identification mark by means of a

band at the mouth end. The retail packaging are preferably stored in a humidor with 70 percent relative

humidity and 21°C temperature.

6 MARKING

6.1 The following particulars shall be legibly and indelibly marked on each retail package in addition to the

declarations as required under any other applicable statutory rules and regulations:

a) Name and address of the manufacturer;

b) Brand name or trade mark, if any;

c) Maximum retail price;

d) Net quantity;

e) Date of manufacture or date code;

f) Any other marking required under the Legal Metrology (Packaged Commodities) Rules, 2011; and

g) Statutory health warnings in the manner and in accordance with the provisions of the rules and

regulations framed under the Cigarettes and Other Tobacco Products Act, 2003 (COTPA).

4

6.2 BIS Certification Marking

The product may also be marked with the Standard Mark

6.2.1 The use of the Standard Mark is governed by the provisions of Bureau of Indian Standards Act, 1986 and

the Rules and Regulations made thereunder. The details of conditions under which the licence for the use of

Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian

Standards.

7 SAMPLING

Drawing of representative samples of the material and the criteria of conformity shall be as prescribed in

Annex B of this standard.

8 TESTS

8.1 Tests shall be carried out as prescribed in 3.3, 3.4 and 3.5 and col 4 of Table 1.

8.2 Quality of Reagents

Unless specified otherwise, pure chemicals and distilled water shall be employed in tests.

NOTE ‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the results of analysis

ANNEX A

(Clause 3.4)

EXAMINATION FOR FREEDOM FROM TOBACCO BEETLE

A-1 PROCEDURE

A-1.1 Take 5 cigars and visually examine the surface of each for the presence of any borings caused by tobacco

beetles. Cut open these cigars one by one and separate the tobacco layers on a large clean white sheet of paper.

A-1.2 Examine the tobacco carefully for the presence of Lasioderma serricorne (tobacco beetle) in all its stages,

that is larval, pupal and alive or dead adult, either visually or with the help of a hand lens (magnification 10X).

A-1.3 Reporting



b) Date of test;

c) If found free of beetles, report as 'Free from beetle attack - Sample passes the test '; and

d) If beetles are present, report as 'Beetle present - Sample fails'.

ANNEX B

(Clause 7)

SAMPLING OF CIGAR

B-1 GENERAL REQUIREMENTS OF SAMPLING

B-1.0 In drawing, preparing, storing and handling samples, the following precautions and directions shall be

observed.

B-1.1 Precautions shall be taken to draw the samples so as to protect the sample, the material being sampled and

the receptacles for samples from loss or gain of moisture and from adventitious contamination.

5

B-1.2 The samples shall be placed in clean and dry receptacles. The receptacles shall be sealed airtight after

filling and marked with full details of sampling, date of manufacture, name of the manufacturer and other

important particulars of the consignment.

B-1.3 Samples shall be stored in such a manner that the conditions of storage do not unduly affect the quality of

the material.

B-1.4 Sampling shall be done by a person agreed to between the buyer and the vendor and in the presence of the

buyer (or his representative) and the vendor (or his representative).

B-2 SCALE OF SAMPLING

B-2.1 All the bulk containers in a single consignment of the material pertaining to the same brands shall

constitute a lot. If the consignment is declared to consist of different brands, the bulk containers belonging to

the same brand shall be grouped together to constitute separate lots.

B-2.1.1 Samples shall be tested for each lot for ascertaining conformity of the materials to the requirements of

this specification.

B-2.2 The number of bulk containers to be selected from the lot shall depend on the size of lot and shall be in

accordance with Table 2.

Table 2 Number of Bulk Containers to be selected for Sampling

(Clause B-2.2)

Lot size to be selected Number of Bulk Containers

(N) (n)

(1) (2)

Below 5 2

6 to 10 3

Over 10 4

B-2.3 These bulk containers shall be chosen at random and for this purpose some random number table

(see IS 4905) as agreed to between the buyer and the vendor shall be used. In case such a table is not available,

the following procedure shall be adopted.

B-2.3.1 Arrange all the bulk containers in the lot in one order and count them as 1, 2, 3, up to r and so on, every

rth

bulk container thus counted shall be withdrawn to give a sample for test, where r = N /n (see Table 2).

N being the number of bulk containers in the lot and n being the number of bulk containers to be chosen.

If r comes out to be a fractional number, its value shall be taken as equal to the integral part of it.

B-3 PREPARATION OF SAMPLES

B-3.1 Individual Sample

The number of packets to be taken at random from each selected bulk container shall be sufficient so as to give

about 300 g of the material. The material so taken shall be mixed, 150 g of the same shall be taken, crushed into

small pieces, thoroughly mixed together and then divided into three equal parts. Each part shall constitute an

individual sample representing the bulk container and shall be transferred immediately to thoroughly clean and

dry receptacles and sealed air-tight. The receptacles shall be labelled with the particulars given under B-1.2.

B-3.1.1 The individual samples so obtained from the lot shall he divided into three sets in such a way that every

set has an individual sample representing each selected bulk container. One of these sets shall be marked for the

buyer, another for the vendor and the third for the referee and all the three sets shall bear the seals of the buyer

and the vendor.

B-3.2 Composite Sample

From the portion of the material left over after preparing the individual sample (see B-3.1), equal quantities of

material shall be taken for each selected container and well mixed together to form a composite sample of about

150 g for the lot.

6

B-3.2.1 The composite sample shall be divided into three equal parts, one for the buyer, another for the vendor

and the third for the referee and all the three samples shall bear the seals of the buyer and the vendor.

B-3.3 Referee Sample

Referee sample shall consist of a set of individual sample (see B-3.1) and a composite sample (see B-3.2)

marked for this purpose and shall bear the seals of the buyer and the vendor. These shall be kept at a place

agreed to between the two.

B-4 NUMBER OF TESTS

B-4.1 Tests for the determination of oven moisture content, total alkaloids as nicotine and total ash shall be

conducted on each of the individual sample (see B-3.1)

B-4.2 Tests for the determination of the remaining characteristic shall be conducted on the composite sample

(see B-3.2)

B-5 CRITERIA OF CONFORMITY

B-5.1 A lot shall be declared as conforming to the specification when:

a) each of the test results of the individual samples for oven moisture content, total alkaloids as nicotine,

and total ash satisfies the corresponding requirement specified in Table 1. If, however, one or more test

results do not satisfy the respective requirement, the conformity of the lot shall be ascertained in

accordance with B-5.1.1.

b) The test results on the composite samples for the remaining requirement shall satisfy the corresponding

requirement as given in 3.2, 3.3, 3.4 and 3.5.

B-5.1.1 In case one or more of the test results do not satisfy the requirements for oven moisture content, total

alkaloids as nicotine and total ash, the following procedure shall be adopted for determining conformity of the

material in respect of these characteristics.

The mean and the range of the corresponding test results shall be calculated as:

Mean (X) = Sum of the test results

Number of the test results

Range (R) = Difference between the maximum and the minimum of the test results.

The appropriate expression as shown in col 6 of Table 3 shall be calculated. If the values of these expressions

satisfy the relevant condition as given in col 6 of Table 3, the lot shall be deemed to have satisfied the

requirements for moisture content, total alkaloids as nicotine and total ash.

Table 3 Criteria for Conformity

(Clause B-5.1.1)

Sl

No.

Characteristic

Test

Results

1,2,3…n

Average

Range

Criterion for

Conformity

(1) (2) (3) (4) (5) (6)

i) Oven moisture content X1 R1 X1±0.4 R1 ≤ 16

ii) Total alkaloids as

nicotine X2 R2

X2 + 0.4 R2 ≤ 3.5

iii) Total ash X3 R3 X3 + 0.4 R3 ≤ 25.0

1

For BIS Use Only



CIGARS AND CHEROOTS SPECIFICATION

PART 2 CHEROOTS

(Third Revision of IS 1769 Part 2) ICS No. 65.160





FOREWORD


A number of brands of cheroots are manufactured in the country depending upon the leaf used, processing

techniques employed and their finish. The range of types of cheroots available in the country is very wide

and it was necessary to lay down a standard to enable the Indian consumer to get a product of assured quality.

This standard was originally published in 1961 and subsequently revised in 1973 and 1994. This revision has

been undertaken to update the requirements of cheroots on the basis of the advancement in analytical science

and prevailing packaging and tobacco rules and regulations.





1 SCOPE

1.1 This standard prescribes requirements, methods of sampling and test for cheroots.

1.2 It does not cover the requirements of flavour and aroma of cheroots.

2 REFERENCES





IS No. Title










2

3 REQUIREMENT

3.1 Description

3.1.1 Cheroot is a smoking article made entirely of tobacco specially grown and processed for cheroots.

Cheroots shall be made from filler and wrapper tobaccos. Pieces of filler tobacco are hand-rolled in the wrapper

tobacco. For keeping the wrapper in position, the end portions shall be either twisted or tied with cotton thread

with or without a paper label sticker or a band. Cheroots can taper from one end to the other or can be uniformly

cylindrical with both ends open.

3.1.2 Cheroot Tobaccos

Cheroot tobaccos are of distinct variety grown in identified areas having required soil and climatic conditions.

Different types of Indian tobaccos are described in IS 10335. The tobacco leaf is air-cured and then fermented.

The fermented tobacco leaves are stemmed to remove the midrib, only lamina is used in cheroots.

3.1.2.1 Filler tobacco A particular grade or a blend of filler tobaccos is used to provide the desired aroma and

flavour.

3.1.2.2 Wrapper tobacco Wrapper leaf, as the name suggests, wraps the roll of filler tobacco. Wrapper leaf

shall be free of any blemish. All cheroots in a packet shall have the same colour, hence the wrapper leaf shall be

uniform in colour.

3.2 Length

The length of cheroots shall be as agreed between the buyer and vendor and shall be measured using a scale of

0.5 mm accuracy and expressed in mm.

3.3 Mean Mass

The mass of cheroots shall be as agreed between the buyer and vendor. It shall be determined by weighing a few

cheroots using an analytical balance having a resolution of 0.001 g and calculating the mean mass.

3.4 Freedom from Tobacco Beetle Attack

Cheroots shall be free from any tobacco beetle attack when examined by the method prescribed in Annex A.

3.5 The material shall also conform to the requirements specified in Table 1.

Table 1 Requirements for Cheroots

(Clause 3.5)

Sl

No.


Ref to

(1) (2) (3) (4)



mass, Max

3.5 8 of IS 5643 or

IS 16132 or IS 16026


iv) Silicated residues insoluble in hydrochloric acid

(on dry basis), percent by mass, Max

5.0 IS 16236

4 SORTING

After manufacture, cheroots shall be graded according to the colour of the wrapper. Cheroots of uniform colour

shall be packed in one packet.

5 PACKING

Number of cheroots shall be packed in retail containers of wood, tin, or cardboard box or in a paper bundle as

agreed to between the buyer and the vendor.

3

6 MARKING






d) Net quantity;








the Rules and Regulations made thereunder. The details of conditions under which the licence for the use of


Standards.

7 SAMPLING

Drawing of representative samples of the material and the criteria of conformity shall be as prescribed in

Annex B to this standard.

8 TESTS

8.1 Tests shall be carried out as prescribed in 3.2, 3.3, 3.4, 3.5 and col 4 of Table 1.


Unless specified otherwise, pure chemicals and distilled water shall be employed in tests.

NOTE — 'Pure chemicals' shall mean chemicals that do not contain impurities which affect the results of analysis.

ANNEX A

(Clause 3.4)

EXAMINATION FOR FREEDOM FROM TOBACCO BEETLE

A-1 PROCEDURE

A-1.1 Take 5 cheroots and visually examine the surface of each for the presence of any borings caused by

tobacco beetles. Cut open these cigars one by one and separate the tobacco layers on a large clean white sheet

of paper.

A-1.2 Examine the tobacco carefully for the presence of Lasioderma serricorne (tobacco beetle) in all its stages,

that is larval, pupal and alive or dead adult, either visually or with the help of a hand lens (magnification 10X).

A-1.3 Reporting



b) Date of test;

c) If found free of beetles, report as 'Free from beetle attack - Sample passes the test '; and

d) If beetles are present, report as 'Beetle present - Sample fails'.

4

ANNEX B

(Clause 7)

SAMPLING OF CHEROOTS

B-1 GENERAL REQUIREMENTS OF SAMPLING

B-1.0 In drawing, preparing, storing and handling samples, the following precautions and directions shall be

observed.

B-1.1 Precautions shall be taken to draw the samples so as to protect the sample, the material being sampled and

the receptacles for samples from loss or gain of moisture and from adventitious contamination.

B-1.2 The samples shall be placed in clean and dry receptacles. The receptacles shall be sealed airtight after

filling and marked with full details of sampling, date of manufacture, name of the manufacturer and other


B-1.3 Samples shall be stored in such a manner that the conditions of storage do not unduly affect the quality of

the material.

B-1.4 Sampling shall be done by a person agreed to between the buyer and the vendor and in the presence of the

buyer (or his representative) and the vendor (or his representative).

B-2 SCALE OF SAMPLING

B-2.1 All the bulk containers in a single consignment of the material pertaining to the same brands shall

constitute a lot. If the consignment is declared to consist of different brands, the bulk containers belonging to

the same brand shall be grouped together to constitute separate lots.

B-2.1.1 Samples shall be tested for each lot for ascertaining conformity of the materials to the requirements of

this specification.

B-2.2 The number of bulk containers to be selected from the lot shall depend on the size of lot and shall be in

accordance with Table 2.

Table 2 Number of Bulk Containers to be selected for Sampling

(Clause B-2.2)


(N) (n)

(1) (2)

≤ 5 2

6 to 10 3

> 10 4

B-2.3 These bulk containers shall be chosen at random and for this purpose some random number table

(see IS 4905) as agreed to between the buyer and the vendor shall be used. In case such a table is not available,

the following procedure shall be adopted.

B-2.3.1 Arrange all the bulk containers in the lot in one order and count them as 1, 2, 3, up to r and so on, every

rth

bulk container thus counted shall be withdrawn to give a sample for test, where r = N /n (see Table 2).

N being the number of bulk containers in the lot and n being the number of bulk containers to be chosen.

If r comes out to be a fractional number, its value shall be taken as equal to the integral part of it.

B-3 PREPARATION OF SAMPLES

B-3.1 Individual Sample

The number of packets to be taken at random from each selected bulk container shall be sufficient so as to give

about 300 g of the material. The material so taken shall be mixed, 150 g of the same shall be taken, crushed into

small pieces, thoroughly mixed together and then divided into three equal parts. Each part shall constitute an

5

individual sample representing the bulk container and shall be transferred immediately to thoroughly clean and

dry receptacles and sealed air-tight. The receptacles shall be labelled with the particulars given under B-1.2.

B-3.1.1 The individual samples so obtained from the lot shall he divided into three sets in such a way that every


buyer, another for the vendor and the third for the referee and all the three sets shall bear the seals of the buyer

and the vendor.

B-3.2 Composite Sample

From the portion of the material left over after preparing the individual sample (see B-3.1), equal quantities of

material shall be taken for each selected container and well mixed together to form a composite sample of about

150 g for the lot.

B-3.2.1 The composite sample shall be divided into three equal parts, one for the buyer, another for the vendor

and the third for the referee and all the three samples shall bear the seals of the buyer and the vendor.

B-3.3 Referee Sample

Referee sample shall consist of a set of individual sample (see B-3.1) and a composite sample (see B-3.2)

marked for this purpose and shall bear the seals of the buyer and the vendor. These shall be kept at a place

agreed to between the two.

B-4 NUMBER OF TESTS

B-4.1 Tests for the determination of oven moisture content, total alkaloids as nicotine and total ash shall be

conducted on each of the individual sample (see B-3.1)

B-4.2 Tests for the determination of the remaining characteristic shall be conducted on the composite sample

(see B-3.2)

B-5 CRITERIA OF CONFORMITY

B-5.1 A lot shall be declared as conforming to the specification when:

a) each of the test results of the individual samples for oven moisture content, total alkaloids as nicotine,

and total ash satisfies the corresponding requirement specified in Table 1. If, however, one or more test

results do not satisfy the respective requirement, the conformity of the lot shall be ascertained in

accordance with B-5.1.1.

b) The test results on the composite samples for the remaining requirement shall satisfy the corresponding

requirement as given in 3.2, 3.3, 3.4 and 3.5.

B-5.1.1 In case one or more of the test results do not satisfy the requirements for oven moisture content, total

alkaloids as nicotine and total ash, the following procedure shall be adopted for determining conformity of the

material in respect of these characteristics.

The mean and the range of the corresponding test results shall be calculated as:

Mean (X) = Sum of the test results

Number of the test results

Range (R) = Difference between the maximum and the minimum of the test results.

The appropriate expression as shown in col 6 of Table 3 shall be calculated. If the values of these expressions

satisfy the relevant condition as given in col 6 of Table 3, the lot shall be deemed to have satisfied the

requirements for moisture content, total alkaloids as nicotine and total ash.

6

Table 3 Criteria for Conformity

(Clause B-5.1.1)

Sl

No.

Characteristic

Test

Results

1,2,3…n

Average

Range

Criterion for

Conformity

(1) (2) (3) (4) (5) (6)

i) Oven moisture content X1 R1 X1±0.4 R1 ≤ 16

ii) Total alkaloids as

nicotine X2 R2

X2 + 0.4 R2 ≤ 3.5

iii) Total ash X3 R3 X3 + 0.4 R3 ≤ 25.0

1

For BIS Use Only




METHODS OF TEST FOR TOBACCO

(Third Revision of IS 5643) ICS No. 65.160





FOREWORD


The methods of test prescribed in this standard are based on the methods followed by the manufacturers,

consumers and testing authorities concerned in the country. This standard will ensure uniformity in test

methodology for assessing the quality of tobacco products.

This standard was originally published in 1970 and subsequently revised in 1989 and 1999 and amended in

2005. In the second revision, provisions of conditioning of atmosphere as given in ISO 3402 : 1991 ‘Tobacco

and tobacco products Atmosphere for conditioning and testing’ were included and provisions of

IS 7753 : 1989 ‘Method for expression of analytical test results of tobacco (first revision)’ were merged.

Consequently, with the publication of second revision of this standard, IS 7753 was withdrawn. This revision

has been undertaken to update various test methods in the standard in light of new scientific knowledge and

advances in analytical techniques. The provisions of determination of total alkaloids by spectrometric method

have been deleted in this revision in view of adoption of corresponding ISO Standard as Indian Standard under

dual numbering system.

In reporting the result of a test or analysis made in accordance with this standard, is to be rounded off, it shall be

done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)'. The number of

significant places retained in the rounded off value should be the same as that of the specified value in this

standard.

1 SCOPE

This standard prescribes the methods of test for tobacco.

2 REFERENCES





IS No. Title

5194 : 1969 Method for determination of nitrogen Kjeldahl method

9379 : 2008 Tobacco and tobacco products Determination of water content

/ISO 6488 : 2004 Karl fischer method (third revision)

16121 : 2013 Tobacco and tobacco products Atmosphere for conditioning and testing

/ISO 3402 : 1999





2

Doc: FAD 04 (2575)F Draft Indian Standard Tobacco and tobacco products — Determination of water

content — Gas-chromatographic method (Adoption of ISO 16632:2013)-under print

3 QUALITY OF REAGENTS

Unless specified otherwise, pure chemicals and distilled shall be employed in tests.

NOTE —‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the experimental results.

4 SAMPLE PREPARATION

4.1 Draw sufficient amount of the test sample for the tests to be carried out. Keep aside 50 g of the sample for

the tests given under 6 and 7. If required, reduce the sample particle size to about 1 mm by grinding.

NOTES

1 Grinding, cutting or undue handling of the sample can cause change in the moisture content of the sample. Moisture content should be

carried out on sample as received as far as possible.

2 If the test sample has higher moisture than 15 percent, it can not be ground and should be dried in air or at 40C to reduce the moisture

to about 10 percent or less.

3 Grinding can also cause changes in the sample due to heat generated. Hence, due care should be taken while grinding not to allow unnecessary high heat.

4.2 Storage

Sample as received and/or after particle size reduction and homogenization, should be packed in air-tight

containers and stored in conditions that will minimize deterioration and maintain sample integrity for any

follow-up analytical work. For long term storage, sample containers shall be stored below 4C.

5 CONDITIONING AND TESTING ATMOSPHERE

The sample may be subjected to conditioning if required by the provisions of the applicable standards or as

agreed to between the buyer and seller. It is not applicable in the case of test methods for which particular test

conditions are laid down elsewhere. The conditioning and testing atmospheres and duration of conditioning shall

be as prescribed in IS 16121.

6 DETERMINATION OF OVEN MOISTURE

6.1 Principle

Tobacco loses mass on heating due to the loss of moisture and some volatiles. If the heating is done under

strictly controlled set of parameters, this loss of mass is termed oven moisture in common tobacco terminology.

This is also referred to as oven volatiles and loss on heating in some tobacco circles.

NOTE For the determination of exact water in tobacco and tobacco products, see IS 9379 and FAD 04(2575)F.

6.2 Apparatus

Usual laboratory apparatus and, in particular, the following:

6.2.1 Dish, made of aluminium, stainless steel, silica or porcelain and provided with a perforated cover.

The diameter of the dish shall be at least 50 mm and the depth not more than 40 mm.

6.2.2 Oven, fitted with a ventilator and means for forced internal circulation of air and maintained at a

temperature of 100±0.5C.

6.2.3 Analytical balance, with a resolution of 0.0001g.

6.3 Procedure

Place about 10 g of the material in a tared dish, close it with the perforated cover, weigh, and place it in the oven

which shall previously have been brought to a temperature of 100±0.5C. Maintain this temperature in the oven

3

for 15 h. Remove the dish and allow it to cool in a desiccator. Weigh the dish with cover and the contents and

note the weight of the material.

6.4 Calculation

Oven moisture, percent by mass = 100 (W1 - W2)

W1

where,

W1 = mass, in g, of the material taken for the test; and

W2 = mass, in g, of the material after heating.

7 EXAMINATION FOR FREEDOM FROM WEEVIL ATTACK

7.1 Procedure

Take about 10 g of the material (see 4) on a large, clean sheet of paper. Loosen the lumps of the material and

examine for the presence or absence of weevil (dead and alive) by naked eye (corrected for abnormal vision).

A hand lens (magnification 10X) may also be used. In case a larger magnification is used, this shall be stated in

the test report.

8 DETERMINATION OF TOTAL NICOTINE ALKALOIDS AS NICOTINE

8.1 Principle

Determination of total nicotine alkaloids may be carried out either gravimetrically by silico-tungstic acid

method (see 8.2) or by spectrophotometric method (see IS 16132) or by continuous flow analysis method

(see IS 16026). Nicotine alkaloids complex with silico-tungstic acid in acidic medium to form insoluble

nicotine silico-tungstate. The mass of the precipitate is determined by filtration using an ashless filter paper in

combination with incineration or a sintered glass crucible in combination with oven-drying

8.2 Silica-Tungstic Acid Method

8.2.1 Apparatus

Normal laboratory apparatus in particular the following:

8.2.1.1 Kjeldahl flask, 500 ml capacity.

8.2.1.2 Distillation assembly The assembly apparatus consists of a distillation flask 500 ml (Kjeldahl flask or

a round-bottom flask) of suitable capacity, having a provision for fitting a splash head and an inlet tube for

steam reaching the bottom of the flask. The free outlet of the splash head is connected to a well-cooled

condenser. the delivery tube of which dips below the surface of dilute hydrochloric acid contained in a receiving

Erlenmeyer flask. It should also be possible to heat the distillation flask, using a burner, heating mantle or some

such heating device, to maintain a constant liquid level during distillation.

8.2.1.3 Crucible, silica or platinum for incineration

8.2.1.4 Laboratory oven, capable of maintaining 120±5C.

8.2.1.5 Sintered glass crucible Gooch type, of porosity 2 (40 m to 100 m).

8.2.1.6 Filter flank (Buchner flask)

8.2.1.7 Vacuum source

8.2.1.8 Desiccator, containing an effective drying agent.

8.2.1.9 Analytical balance, with a resolution of 0.0001 g.

8.2.1.10 Bunsen burner

8.2.2 Reagents

8.2.2.1 Liquid paraffin

8.2.2.2 Sodium hydroxide solution, aqueous 30 percent (m/v).

8.2.2.3 Sodium chloride

8.2.2.4 Phenolphthalein indicator solution, 0.2 percent (m/v) Dissolve 0.2 g of phenolphthalein in 60 ml of

rectified spirit and dilute to 100 ml with water.

8.2.2.5 Dilute hydrochloric acid, 1 : 4 and 1 : 1000 (v/v).

4

8.2.2.6 Silico-tungstic acid solution Dissolve 120 g of silico-tungstic acid (4H2O, SiO2, 12WO3, 22H2O) in

100 ml water and dilute to one litre . The solution should be free from cloudiness and green colour.

NOTE The silico-tungstic acid should be white or pale yellow crystals free from green colour. Of the silico-tungstic acids, 4H2O, SiO2, 10WO3, 3 H2O, and 4H2O, SiO2, 12WO3, 20H2O should not be used as these do not give crystalline precipitate with

nicotine.

8.2.2.7 Methyl orange indicator solution, 0.04 percent (m/v) in aqueous ethyl alcohol (20 percent by volume).

8.2.3 Procedure

8.2.3.1 Weigh accurately a quantity of the material that shall contain preferably a minimum of 0.1 to 1 .0 g of

nicotine in a suitable tared vessel. Quantitatively, transfer the weighed material to the distillation flask (a 500 ml

Kjeldahl flask or a round bottom flask) using water to wash the last traces of the material into the flask. If

necessary, add to the contents of Kjeldahl flask or a round bottom the distillation flask a small amount few drops

of liquid paraffin to prevent frothing during distillation and a few small pieces of pumice stone to prevent

bumping. Add 10 ml of sodium hydroxide solution (see 8.2.2.2) using and a few drops of phenolphthalein as

indicator. Fit the mouth of the Kjeldahl flask with a two holed, rubber stopper through which pass the stem of a

trap bulb and an inlet tube for steam. Connect the free end of the trap bulb to a condenser. Assemble the

distillation unit with the receiving flask containing 10 ml of dilute hydrochloric acid (1 : 4), the delivery end of

the condenser dipping well below the surface of the liquid in the receiving flask.

Connect the steam inlet tube to the source of steam and pass steam in the distillation flask to start distillation.

Distil rapidly with the current of steam. When the distillation is well under way, heat the distillation Kjeldahl

flask using Bunsen burner to reduce the volume of contents of the flask as far as practicable without causing

bumping or undue separation of insoluble matter externally to maintain constant liquid level in the flask during

distillation. Continue the distillation until a small quantity of the distillate shows no cloudiness or opalescence

when treated with a drop of silico-tungstic acid and a drop of dilute hydrochloric acid (1 : 4). Confirm the

alkalinity of the residue in the distillation Kjeldahl flask with phenolphthalein indicator solution.

Reduce the volume of the distillate by concentrating it on a steam boiling water bath (see Note) and make up the

volume of the concentrated distillate to a convenient volume in a graduated flask with water at room

temperature. Mix the contents of the graduated flask thoroughly and filter through a dry filter paper if it is not

clear. Collect the filtrate in a convenient flask. Test a portion of this filtrate with methyl orange indicator to

confirm its acidity.

NOTE — By heating on a steam-boiling water bath, the nicotine content of the distillate is not affected.

8.2.3.2 Pipette an aliquot (see Note 1) of the filtrate, containing about 0.1 g of nicotine into a beaker and add at

the rate of 3 ml of dilute hydrochloric acid (1 : 4) for each 100 ml of the aliquot and one ml of silico-tungstic

acid solution for every 0.01 g of nicotine supposed to be present in the aliquot. Stir the contents of the beaker

thoroughly, heat it on a water-bath for about 30 minutes till the precipitate settles down and allow to stand

overnight in a refrigerator. Before filtering, stir the contents of the beaker to see that the precipitate settles down

quickly and is in a crystalline form.

NOTES 1 If the nicotine content of the material is very low, an aliquot containing at least 0.0 1 g of nicotine should be used.

2 The mass of the precipitate can be determined by collecting the precipitate on a filter paper followed by incineration (see 8.2.4) or by

collecting on a sintered glass crucible and drying (see 8.2.5).

8.2.4 Filter Paper-Incineration Method

8.2.4.1 Filter the contents of the beaker through an ashless filter paper. Wash all the residue remaining in the

beaker on to the filter using dilute hydrochloric acid (1 : 1000) at room temperature. Wash the filter paper with

dilute hydrochloric acid (1 : 1000) until a few millilitres of the filtrate do not produce a precipitate or

opalescence when tested with a few drops of the distillate containing nicotine.

8.2.4.2 Dry the crucible (see 8.2.1.3) in the laboratory oven until it shows constant weight (±1 mg). Store the

crucible in a desiccator (see 8.2.1.8).

8.2.4.3 Transfer the filter paper containing the precipitate to the tared crucible (see 8.2.4.2), Place the crucible

on a silica triangle resting on a tripod, heat gently at first to dry and then ignite the filter paper with a Bunsen

5

burner completely to ash until all carbon is oxidized. Finally, heat the platinum crucible over a Bunsen burner

for not more than 10 minutes. Cool the crucible in a desiccator (see 8.2.1.8) and weigh. Repeat the heating

process until a constant weight (±1 mg) is obtained.

NOTE If the nicotine content of the material is very low, an aliquot containing at least 0.0 1 g of nicotine should be used.

8.2.4.2 Calculation

Total alkaloid as nicotine (on dry basis), percent by mass = 0.1141 (W1 x V1)

(W2 x V2)(100 - M)

where,

W1 = mass, in g, of the residue in the crucible;

V1 = total volume, in ml, of the concentrated distillate after making up the volume (see 8.2.3.1);

W2 = mass, in g, of the material taken for steam distillation;

V2 = volume, in ml, of the aliquot of the filtrate taken for the precipitation (see 8.2.3.2);

M = moisture, percent by mass (see 6.4).

8.2.5 Sintered Glass Crucible Method

8.2.5.1 Dry the sintered glass filter crucible in a laboratory oven to constant mass (±1 mg). Store in a desiccator.

Weigh to the nearest 0.0001 g, the dried sintered glass crucible and filter the precipitate directly into the glass

filter using a Buchner flask connected to a vacuum source. Ensure that all the precipitate Is removed from the

sides of the beaker and the glass stirring rod by rinsing three times with hydrochloric acid solution using 15 ml

each time and transferring the rinse to the crucible. Discard the washings.

Rinse with a further aliquot of hydrochloric acid (up to 400 ml may be required) which should be collected and

tested with a few drops of nicotine solution to ensure that no opalescence occurs i.e. all silico-tungstic acid has

been removed. Dry the sintered glass crucible with the precipitate in the laboratory oven, cool in the desiccator

and weigh to the nearest 0,0001 g. Place the crucible back in the oven for 1 h, allow to cool and reweigh. Repeat

until a constant weight ±1 mg is obtained.

8.2.5.2 Calculation

Total alkaloid as nicotine (on dry basis), percent by mass = 0. 1012 (W1 x V1)

(W2 x V2)(100 - M)

where,

W1 = mass, in g, of the residue in the crucible;

V1 = total volume, in ml, of the concentrated distillate after making up the volume (see 8.2.3.1);

W2 = mass, in g, of the material taken for steam distillation;

V2 = volume, in ml, of the aliquot of the filtrate taken for the precipitation (see 8.2.3.2);


8.3 Spectrophotometric Method

Total nicotine alkaloids can be determined by a spectrometric method prescribed in IS 16132.

8.4 Continuous Flow Analysis Method

Total nicotine alkaloids can also be determined by continuous flow analysis as prescribed in IS 16026.

8.5 Repeatability

Duplicate determination should agree within 0.05 percent by mass of nicotine. If not, further duplicate

determinations should be made until this requirement is fulfilled.

6

9 DETERMINATION OF TOTAL NITROGEN

9.1 Principle

Total nitrogen is the amount of both organic and inorganic nitrogen present in the tobacco sample. The sample is

first pre-digested with reducing agents to convert inorganic nitrogen (nitrate and nitrite) into ammonium salt

followed by digesting with oxidizing agents to convert all nitrogenous matter into ammonium sulphate.

Ammonia in the Kjeldhal digest is quantitatively liberated by steam distillation, analyzed and expressed as total

nitrogen. The ammonia concentration in the distillate can be determined using titrimetric, colorimetric or

specific ion electrode determination methods. The method prescribed here employs the titrimetric method.

9.2 Apparatus

Usual laboratory apparatus and, in particular, the following:

9.2.1 Kjeldahl digestion flask, 500 ml or of suitable capacity.

9.2.2 Kjeldahl distillation apparatus with distillation flask of suitable capacity (see IS 5194)

NOTE — Kjeldahl apparatus from micro to macro scale and consisting of digestion and distillation in one unit are available commercially. These units work satisfactorily and can be used following the user instructions provided by the supplier.

9.4 Procedure

9.4.1 Digestion

Transfer about 1 g of sample (see 4) accurately weighed to 0.0001g, in a 500 ml Kjeldahl digestion flask

containing 1 g of salicylic acid and add 30 ml of concentrated sulphuric acid (see 9.3.1) rinsing the neck of the

flask. Shake until thoroughly mixed and allow to stand, shaking frequently, for at least 30 minutes. Add 5 g of

sodium thiosulphate and heat the solution for 5 minutes. Cool and add a mixture of 10 g potassium sulphate or

anhydrous sodium sulphate and 1 g copper sulphate carefully to avoid sticking of the mixture in the neck of the

flask. Heat very gently keeping the flask in an inclined position until foaming ceases. Increase the heat till acid

boils briskly, continue boiling till the digest becomes clear and green and digest for a few more minutes (total

digestion time is approximately two hours).

NOTES

1 Ready-made salt catalyst mixtures available commercially can also be used following the instructions provided by the supplier.

2 This digesting operation shall be carried out in a fume hood .

9.4.2 Distillation

After cooling, dilute with 200 ml of water. Transfer the contents quantitatively to the distillation flask by rinsing

the Kjeldhal flask repeatedly. Add a few pieces of granulated zinc or pumice stone to prevent bumping. Add a

few drops of phenolphthalein indicator (see 9.3.8). Assemble the Kjeldahl distillation unit. Connect the

receiving Erlenmeyer flask or beaker containing 50 ml of 4 percent boric acid solution (see 9.3.10) and a few

drops of 0.5 ml mixed indicator (see 9.3.9), ensuring that the delivery end of the condenser is below the level

of the liquid in the receiving flask. Add gradually 100 ml of sodium hydroxide solution (see 9.3.7) through the

funnel to make the contents thoroughly alkaline as indicated by the phenolphthalein indicator. Heat the

distillation flask to boiling and distil about 150 ml of the distillate in the receiving flask. Lower the receiving

flask to raise the delivery tube above the liquid, distil further for a few seconds. Rinse the tube with water into

the flask. Remove the flask.

9.4.3 Titration

The content in the receiving flask is titrated with 0.1 N sulphuric acid (see 9.3.2), the end point in case of the

mixed indicator, being the colour turning from green to pink and in the case of Sher indicator from blue to pale

pink/yellow.

9.4.4 Carry out a blank determination using all reagents in the same quantities but without the material to be

tested.

7

9.5 Calculation

Total nitrogen, percent by mass (on dry basis) = (V1 - Vo) N 140

W (100 – M)

where,

Vo = volume, in ml, of standard 0.1 N sulphuric acid solution used to titrate the blank distillate;

V1 = volume, in ml, of standard 0.1 N sulphuric acid solution used to titrate the sample distillate;

N = normality of standard sulphuric acid solution;

W = mass in g, of the material taken for the test; and


10 DETERMINATION OF TOTAL ASH

10.1 Procedure

10.1.1 Accurately weigh about 10 g of the material (see 4) into a tared 9 cm diameter platinum, porcelain or

silica dish. Carefully dry the material on a burner flame and char it completely until all organic matter is

destroyed. Ignite the charred material by placing the dish in a muffle furnace maintained at a temperature of

550±25°C for 2 h. Cool the dish and weigh. Note the mass of the ash contained in the dish.

10.1.2 Preserve the ash for the determination of acid insoluble ash.

10.1.3 Calculation

Total ash content of the material (on dry basis), percent by mass = 10 000 W1

W2 (100 - M)

where,

W1 = mass, in g, of the ash;

W2 = mass, in g, of the material taken for the test; and

M = moisture content, percent by mass (see 6.4).

11 DETERMINATION OF ACID INSOLUBLE ASH

11.1 Reagents

11.1.1 Dilute Hydrochloric Acid, 1:1 (v/v).

11.1.2 Concentrated Nitric Acid, sp gr 1.42.

11.2 Procedure

11.2.1 Moisten the ash contained in the dish (see 10.1.2) with a few drops of water. Cover the dish and carefully

add 20 ml of dilute hydrochloric acid avoiding loss due to effervescence. Place the covered dish on a water bath

and digest for 20 to 30 minutes. Remove and rinse the cover, add one millilitre of concentrated nitric acid to

oxidize any ferrous salts and evaporate the contents to dryness. Heat for about 30 minutes on water bath to

dehydrate the silica. If necessary, heat for one hour in an oven at 110°C to complete the dehydration. Moisten

the dry salt with 10 ml of dilute hydrochloric acid and 50 ml of water. Heat on water bath until all soluble salts

are in solution. Filter through a filter paper (Whatman no. 44 or equivalent) and collect the filtrate in a 500 ml

volumetric flask. Transfer all the residue to the filter paper and wash several times with hot dilute hydrochloric

acid.

11.2.2 Transfer the filter paper along with the residue to a platinum dish or silica crucible and ignite to bright

red heat. Cool and weigh the material.

11.3 Calculation

Acid insoluble ash (on dry basis), percent by mass = 10 000 W2 - W)

W1 (100 - M)

8

where,

W = mass, in g, of the empty dish;

W1 = mass, in g, of the material taken for the test (see 11.1.1);

W2 = mass, in g, of dish with acid insoluble ash (see 11.2.2); and

M = moisture content, percent by mass (see 6.4).

12 DETERMINATION OF TOTAL CHLORIDES

12.1 Principle

Chloride reacts with silver nitrate to precipitate silver chloride stoichiometrically. The quantity of silver nitrate

exhausted in the reaction is a direct measure of total chlorides present in the sample. The analysis can be done

using potentiometric, iodometric titration or colorometry. The method prescribed here is based on

potentiometric titration.

12.2 Apparatus

12.2.1 pH Meter, equipped with silver and glass electrodes.

12.2.2 Burette, 10 ml capacity, graduated in 0.05 or 0.02 ml, units.

12.3 Reagents

12.3.1 Standard Silver Nitrate Solution, 0.1 N Standardize against potassium chloride as per the procedure

prescribed in 12.4.

12.3.2 Dilute Nitric Acid, 1 : 9 (v/v).

12.4 Procedure

Weigh accurately about 2 g of tobacco sample (see 4) into a 250 ml beaker. Add 100 ml of water, a small

amount in the first instance to wet the tobacco thoroughly and then the remainder. Allow it to stand for at least 5

minutes at room temperature, stirring intermittently. Add 5 ml of dilute nitric acid into the mixture and insert the

clean electrodes. Start magnetic stirrer and continue stirring throughout titration at a rate sufficient to produce

vigorous agitation without sputtering. Titrate with standard silver nitrate solution to the potential previously

established as equivalent point. Determine equivalence point graphically by making several titrations on one or

more tobacco samples. Recheck occasionally and determine when either electrode is replaced. Record the

volume of the titrant.

12.5 Calculation

Total chlorides (on dry basis), percent by mass = V N 354.533

W (100 – M)

where

V = volume, in ml, of silver nitrate solution required for the test;

N = normality of silver nitrate solution;

W = mass, in g, of the sample taken for the test; and

M = percent moisture content (see 6.4).

13 REPORTING

13.1 Basis of Expression of Results

The results of test according to any of the agreed methods shall be reported as a percentage of the moisture-free

mass of the sample.

1

For BIS Use Only



FLAKE TYPE CHEWING TOBACCO (ZARDA) SPECIFICATION






FOREWORD


A number of brands of flake type chewing tobacco (ZARDA) are manufactured in the country depending upon

the leaf tobacco used, the processing technique employed and the admixture of various ingredients used.

The range of brands of Zarda produced in the country is very wide and it was felt necessary to formulate an

Indian Standard.

This standard was originally published in 1963 and subsequently revised in 1973 and 1999 and amended in

2000 and 2012. This revision is being brought out to update its provisions in the light of developments in

analytical methods, current industrial and trade practices, and the prevailing statutory packaging and tobacco

control rules and regulations.

While formulating this standard, necessary consideration has been given to the relevant rules prescribed by the

Government of India under the Food Safety and Standards Act, 2006 and the rules and regulations framed

thereunder and the Legal Metrology (Packaged Commodities) Rules, 2011. This standard is however, subject to

the restriction imposed under these, wherever applicable.





1 SCOPE

This standard prescribes the requirements, method of sampling and test for flake type chewing tobacco

(ZARDA).

2 REFERENCES





IS No. Title

1070 : 1992 Reagent grade water — Specification (third revision)

3110 : 1982 Specification for silver leaf (first revision)








2



3 DESCRIPTION

3.1 Flake type chewing tobacco, commonly known as Zarda, is a preparation made of scented and flavoured

tobacco flakes. It is usually chewed along with betel nut and paan (betel leaf).

3.2 Chewing tobacco blend consists of tobaccos grown in identified areas, specially cured and processed for

chewing purposes. Different types of Indian tobaccos are described in IS 10335. Cured leaf is coarsely

pulverised, sieved through a set of sieves to remove the fine powder and coarser flakes. Flakes of required mesh

size are only used for Zarda. The tobacco blend is mixed with select spices, cardamom, clove, floral essences,

flavours and menthol. Expensive varieties of Zarda also contain saffron and silver foil.

3.3 It may contain approved preservatives as permitted under the Food Safety and Standards Act, 2006 and its

rules and regulations.

4 REQUIREMENTS

4.1 Sliver Foils (Leaf)

Silver foils (leaf) when used shall conform to IS 3110.

4.2 Additives

Any substances, if added, shall be of a nature and purity which are suitable for use as food additives as

permitted under the Food Safety and Standards Act, 2006 and its rules and regulations.

4.3 The material shall also conform to the requirements prescribed in Table 1.

Table 1 Requirements for Flake Type Chewing Tobacco (Zarda)

(Clauses 4.3, 8.1 and A-4)

Sl

No.


Ref to

(1) (2) (3) (4)

i) Oven moisture content, percent by mass, Max 20 6 of IS 5643


mass, Max

4.0 8 of IS 5643 or

IS 16132 or IS 16026




4.0 IS 16236

5 PACKING

The material shall be packed in retail containers made of waxed paper, glassine paper, glass, tinplate or any

other suitable container and permitted laminated pouches which will help in the preservation of moisture and

aroma. The quantity per retail container and the type of container shall be as agreed to between the purchaser

and the vendor. These retail containers may then be packed in bulk container as agreed to between the purchaser

and the manufacturer.

6 MARKING






d) Net quantity;

3










Standards.

7 SAMPLES FOR TESTING

The method of drawing representative samples of the material shall be as prescribed in Annex A or as agreed to

between the purchaser and vendor. The conformity of the material to the requirements of this specification shall

be determined by testing the samples as prescribed in 4 and A-4 of Annex A.

8 TESTS

8.1 Tests shall be carried out as prescribed in 4, col 4 of Table 1 and A-4 of Annex A.


Unless specified otherwise, pure chemicals shall be employed in tests and distilled water (see 1070) shall be

used where the use of water as reagent is intended


ANNEX A

(Clauses 7 and 8)

SAMPLING OF FLAKE TYPE CHEWING TOBACCO (ZARDA)

A-1 GENERAL REQUIREMENTS OF SAMPLING

A-1.0 In drawing, preparing, storing and handling samples, the following precautions and directions shall be

observed.

A-1.1 Precautions shall be taken to draw the samples so as to protect the samples, the material being sampled,

the sampling instruments and the receptacles for samples from loss or gain of moisture and from adventitious

contamination.

A-1.2 The samples shall be placed in clean and dry receptacles. The sample receptacle shall be sealed air tight

after filling and marked with full details of sampling, date of manufacture, name of the manufacturer and other


A-1.3 Samples shall be stored in such a manner that the conditions of storage do not unduly affect the quality of

the material.

A-1.4 Sampling shall be done by a person agreed to between the purchaser and vendor and in the presence of

the purchaser (or his representative) and the vendor (or his representative).

A-2 SCALE OF SAMPLING

A-2.1 All the bulk containers in a single consignment of the material pertaining to the same brands shall

constitute a lot. If the consignment is declared to consist of different brands, the bulk containers belonging to the

same brand shall be grouped together to constitute separate lots.

A-2.1.1 Samples shall be tested for each lot for ascertaining conformity of the materials to the requirements of

this specification.

4

A-2.2 The number of bulk containers to be selected from the lot shall depend on the size of the lot, and shall be

in accordance with Table 2.

A-2.3 These bulk containers shall be chosen at random from the lot and for this purpose some random number

table as agreed to between the purchaser and the vendor shall be used (see IS 4905).

Table 2 Number of Bulk Containers to be Selected for Sampling

(Clause A-2.2)


(N) (n)

(1) (2)

Below 5 2

6 to 10 3

Over 10 4

A-3 PREPARATION OF SAMPLES

A-3.1 Individual Samples

A-3.1.1 The number of retail containers to be taken at random from each selected bulk container shall be

sufficient so as to give about 150 g of the material. The material so taken out shall be mixed together; about 50 g

will be set aside for preparing the composite sample (see A-3.2) and the remaining shall be divided into three

equal parts each of minimum 30 g. Each part shall constitute an individual sample representing the bulk

container from which it was drawn and shall be transferred immediately to thoroughly clean and dry receptacles

and sealed air-tight. The receptacles shall be labelled with the particulars given under A-1.2.

A-3.1.1 The individual samples so obtained from the lot shall be divided into three sets in such a way that every


purchaser, another for the vendor and the third for the referee and all the three sets shall bear the seals of the

buyer and the vendor.

A-3.2 Composite sample

A-3.2.1 From the materials set aside from each selected bulk container (see A-3.1.1), equal quantities shall be

mixed together to form a composite sample of minimum 150 g for the lot.

A-3.2.2 The composite sample (see A-3.2.1) shall be divided into three equal parts. Each part shall constitute a

composite sample representing the lot and shall be transferred immediately to thoroughly clean and dry

receptacles and sealed air-tight. The receptacles shall be labelled with the particulars given under A-1.2 and

marked one for the purchaser, another for the vendor and the third for the referee. All the three samples shall

bear the seals of the purchaser and the vendor.

A-3.3 Referee Sample

Referee sample shall consist of a set of individual samples (see A-3.1.2) and a composite sample (see A-3.2)

marked for this purpose and shall bear the seals of the purchaser and the vendor. These shall be kept at a place

agreed to between the two to be used in case of dispute between the two.

A-4 TESTING PLAN

A-4.1 Tests for the determination of moisture and total nicotine alkaloids (Table 1) shall be conducted on each

of the individual sample in a set (see A-3.1).

A-4.2 Tests for the determination of the remaining characteristics of 4 and of Table 1 shall be conducted in

duplicate on the composite sample (see A-3.2).

A-5 CRITERIA OF CONFORMITY

5

A-5.1 A lot shall be declared as conforming to the specification if the conditions prescribed in A-5.1.1 and

A-5.1.2 are satisfied.

A-5.1.1 The test results on each of the individual samples for determination of requirements given in A-4.1 shall

satisfy the corresponding specification requirements.

A-5.1.2 The test results on the composite samples for the remaining characteristics given in A-4.2 shall satisfy

the corresponding specification requirements.

1

For BIS Use Only



MINCED TYPE CHEWING TOBACCO SPECIFICATION






FOREWORD


A number of brands of minced type chewing tobacco are manufactured in the country depending upon the leaf

tobacco used, the processing technique employed and the admixture of various ingredients used. The range of

brands of chewing tobacco, minced type produced in the country is very wide and it is felt necessary to

formulate an Indian Standard specification.

This standard was originally published in 1965 and subsequently revised in 1973 and 1994. This revision is

being brought out to update its provisions in the light of developments in analytical methods, current industrial

and trade practices, and the prevailing statutory packaging and tobacco control rules and regulations.









1 SCOPE

This standard prescribes the requirements, method of sampling and test for minced type chewing tobacco.

2 REFERENCES





IS No. Title












2

3 DESCRIPTION

3.1 The minced type chewing tobacco (in the form of shreds) is a smokeless tobacco product prepared from

mould-free tobacco which may be spiced and flavoured.

3.2 Chewing type tobaccos are tobaccos specially grown in identified areas, specially cured and processed.

Different types of Indian tobaccos are described in IS 10335. Cured leaf is shredded and sieved to obtain the

desired particle size. A suitable blend of different tobacco grades is mixed with select aromatic spices, floral

essences, flavours and menthol, saffron and silver foil, as required.

4 REQUIREMENT

4.1 Additives

Any substances, if added, shall be of a nature and purity which are suitable for use as food additives as

permitted under the Food Safety and Standards Act, 2006 and its rules and regulations. Flavour ingredients shall

comply with GRAS and FEMA standards.

4.2 Sliver Foil (Leaf)

Silver foil (leaf) when used shall conform to IS 3110.

4.3 The material shall also conform to the requirements prescribed in Table 1.

Table 1 Requirements for Minced Type Chewing Tobacco


Sl

No.


Ref to

(1) (2) (3) (4)



mass, Max

8.0 8 of IS 5643 or

IS 16132 or IS 16026




5.0 IS 16236

5 PACKING

The material shall be packed in retail containers made of waxed paper, glassine paper, glass, tinplate or any

other suitable container and permitted laminated pouches which will help in the preservation of moisture and

aroma. The quantity per retail container and the type of container shall be as agreed to between the purchaser

and the vendor. These retail containers may then be packed in bulk container as agreed to between the purchaser

and the manufacturer

6 MARKING






d) Net quantity;





3






Standards.


The method of drawing samples of the material shall be as prescribed in Annex A or as agreed to between the

purchaser and vendor. The conformity of the material to the requirements of this specification shall be

determined by testing the samples as prescribed in A-4 of Annex A.

8 TESTS

8.1 Tests shall be carried out as prescribed in 4 and col 4 of Table1 and A-4 of Annex A.





ANNEX A

(Clauses 7 and 8)

SAMPLING OF MINCED TYPE CHEWING TOBACCO



observed.



contamination.





the material.

A-1.4 Sampling shall be done by a person agreed to between the purchaser and vendor and in the presence of



A-2.1 All the bulk containers in a single consignment of the material pertaining to the same brands shall



A-2.1.1 Samples shall be tested for each lot for ascertaining conformity of the materials to the requirements of

this specification.

4

A-2.2 The number of bulk containers to be selected from the lot shall depend on the size of the lot, and shall be

in accordance with Table 2.

A-2.3 These bulk containers shall be chosen at random from the lot and for this purpose some random number

table as agreed between the purchaser and the vendor shall be used (see IS 4905).


(Clause A-2.2)


(N) (n)

(1) (2)

Below 5 2

6 to 10 3

Over 10 4

A-3 PREPARATION OF SAMPLES



sufficient so as to give about 150 g of the material. The material so taken out shall be mixed together; about 50 g

will be set aside for preparing the composite sample (see A-3.2) and the remaining shall be divided into three

equal parts each of minimum 30 g. Each part shall constitute an individual sample representing the bulk

container from which it was drawn and shall be transferred immediately to thoroughly clean and dry receptacles

and sealed air-tight. The receptacles shall be labelled with the particulars given under A-1.2.




buyer and the vendor.

A-3.2 Composite sample


mixed together to form a composite sample of minimum 150 g for the lot.

A-3.2.2 The composite sample (see A-3.2.1) shall be divided into three equal parts. Each part shall constitute a

composite sample representing the lot and shall be transferred immediately to thoroughly clean and dry





Referee sample shall consist of a set of individual samples (see A-3.1.2) and a composite sample (see A-3.2)

marked for this purpose and shall bear the seals of the purchaser and the vendor. These shall be kept at a place

agreed to between the two to be used in case of dispute between the two.

A-4 TESTING PLAN

A-4.1 Tests for the determination of moisture and total nicotine alkaloids (Table 1) shall be conducted on each

of the individual sample in a set (see A-3.1).

A-4.2 Tests for the determination of the remaining characteristics of 4 and of Table 1 shall be conducted in

duplicate on the composite sample (see A-3.2).

5








1

For BIS Use Only




HOOKAH TOBACCO PASTE SPECIFICATION

(First Revision of IS 14332) ICS No. 65.160





FOREWORD


Hookah tobacco paste is an admixture of tobacco, molasses, fruit pulps, spices, flavours, etc. Various types of

Hookah tobacco paste are being manufactured in the country for domestic market and for export. Hence, a

standard was formulated laying down certain minimum requirements for Hookah tobacco paste to have a

product of assured quality.

This standard was originally published in 1996 and amended in 2005 and 2012. This revision is being brought

out to update its provisions in the light of developments in analytical methods, current industrial and trade

practices, and the prevailing statutory packaging and tobacco control rules and regulations.





1 SCOPE

This standard prescribes the requirements, method of sampling and test for hookah tobacco paste.

2 REFERENCES





IS No. Title









Doc. FAD 04(2729)C Draft Indian Standard Hookah tobacco, flake type Specification

(second revision of IS 4463)

Doc. FAD 04(2786)C Draft Indian Standard Tobacco and tobacco products Determination of reducing

and total sugars

2

3 DESCRIPTION

Hookah tobacco is a smoking tobacco preparation consisting of tobacco, molasses, fruits extracts and

flavourants. Hookah tobacco is made in two forms - flake [see FAD 04(2729)] and paste. Hookah tobacco

paste is made from native air-cured tobacco varieties mixed with permitted additives like molasses, fruit pulps

and flavours. Hookah tobaccos are distinct air cured varieties of tobaccos grown in identified areas having

required soil and climatic conditions. These tobaccos are specially air cured and processed for use in hookah

tobacco paste. Various hookah tobacco types and varieties are available in the country (see IS 10335). Nearly all

components of the tobacco plant, except its root, are ground and used in different proportions for the preparation

of hookah tobacco paste.

4 REQUIREMENTS

4.1 The material shall comply with the requirements given in Table 1.

Table 1 Requirements for Hookah Tobacco Paste

(Clauses 4.1 and A-4)

Sl

No.


Ref to

(1) (2) (3) (4)



mass, Max

1.0 8 of IS 5643 or

IS 16026

iii) Total sugar (on dry basis), percent by mass, Min 40.0 Doc: FAD 04(2786)

iv) Total ash (on dry basis), percent by mass, Max 15.0 10 of IS 5643

v) Silicated residues insoluble in hydrochloric acid (on


3.5 IS 16236

vi) Total chlorides (on dry basis), percent by mass, Max 2.0 12 of IS 5643

5 PACKING

The material shall be packed in tin plate containers suitably and properly lacquered from inside with food grade

lacquering material. The capacity of a container may either be 1 kg or 4 kg or 16 kg, depending upon the

agreement between the purchaser and the vendor. Each container then shall be packed in 5 to 7 ply corrugated

fibreboard box which then be wrapped with hessian cloth.

6 MARKING






d) Net quantity;










Standards.

3


Samples shall be drawn in accordance with the procedure given in Annex A or as agreed to between the

purchaser and the supplier. The conformity of the material in the lot to the requirements of this specification

shall be determined by testing in accordance with A-4 of Annex A.

8 TESTS

8.1 Tests shall be carried out as prescribed in col 4 of Table1 and A-4 of Annex A.





ANNEX A

(Clause 7)

SAMPLING OF HOOKAH TOBACCO PASTE


A-1.0 In drawing, preparing, storing and handling samples, the following precautions and directions given in

A-1.1 to A-1.4 shall be observed.

A-1.1 Precautions shall be taken to draw the samples so as to protect the sample, the material being sampled,

sampling instruments and the receptacles for samples from loss or gain of moisture and from adventitious

contamination.

A-1.3 The samples shall be placed in clean and dry receptacles. The receptacles shall be sealed air-tight after

filling and marked with full details of sampling, date of packing, name of the manufacturer and other important

particulars of the consignment.

A-1.4 Sample shall be stored in such a manner that the conditions of storage do not unduly affect the quality of

the material.

A-1.5 Sampling shall be done by a person agreed to between the purchaser and the vendor and in the presence of


A-2 SCALEOF SAMPLING

A-2.1 Lot

All the bulk containers of Hookah tobacco paste .in a single consignment of the material pertaining to the same

brand shall constitute a lot. If the consignment is declared to consist of different brands, the bulk containers

belonging to the same brand shall be grouped together to constitute separate lots.

A-2.2 For ascertaining conformity of the materials in a lot to the requirements of this specification, tests shall be

carried out on each lot separately. The number of containers to be selected from the lot shall depend upon the

size of the lot and shall be in accordance with Table 2.

A-2.3 These bulk containers shall be chosen at random and for this purpose some random number tables agreed

to between the purchaser and the vendor shall be used (see IS 4905).

4


(Clause A-2.2)

Lot Size (For 16 kg

Containers)

Number of Bulk

Containers to be Selected

Lot Size (For 1 kg,

4 kg Containers)

Number of Bulk

Containers to be Selected

(N) (n) (N) (n)

Up to 15 3 Up to 15 3

Over 16 4 16 - 50 4

51 - 100 5

101 and above 7

A-3 PREPARATION SAMPLES

On storage of hookah tobacco paste, separation of the liquid and solid constituents may occur. It is necessary to

mix the contents of the container prior to drawing a sample and for this purpose the following procedure is

recommended.

A-3.0 Open the retail container at the edge of the lid or by uncapping or cutting as the case may be.

Reincorporate all the material adhering to the lid/cap/cut-out into the container. Mix the contents thoroughly by

stirring with a spoon or spatula in such a way that the top layers as well as contents of the lower layers are

stirred and mixed well.

A-3.1 Individual Samples.

A-3.1.1 Individual Samples

The number of retail containers to be taken at random from each selected bulk container shall be sufficient so as

to give about 150 g of the material. The material so taken out shall be mixed together; 50 g of the mixed

material shall be set aside for preparing composite sample (see A-3.2); the balance will be divided into three

equal parts of about 30g each. Each part shall constitute an individual sample representing the bulk container

and shall be transferred immediately to thoroughly clean and dry receptacles and sealed air-tight. The

receptacles shall be labelled with the particulars given under A-1.3.




purchaser and the vendor.

3.2 Composite Sample


mixed together to form a composite sample of about 150 g for the lot.

A-3.2.2 The composite sample shall be divided into three equal parts. Each part shall constitute a composite

sample representing the bulk container and shall be transferred immediately to thoroughly clean and dry




A-3.3 Referee Samples

Referee sample shall consist of a set of individual samples (see A-3.1) and a composite sample

(see A-3.2) marked for this purpose and shall bear the seals of the purchaser and the vendor. These receptacles

shall be kept at a place agreed to between the purchaser and the vendor and shall be used in the case of a dispute

between the two.

A-4 TESTING PLAN

A-4.1 Tests for the determination of oven moisture and total alkaloids as nicotine (Table 1) shall be conducted

on each of the individual samples in the set.

5

A-4.2 Tests for determination of the remaining characteristics in 4 and Table 1 shall be conducted in duplicate

on the composite sample.








1

For BIS Use Only




QUIWAM SPECIFICATION

(First Revision of IS 14647) ICS No. 65.160





FOREWORD


Quiwam is a product in paste form similar to chewing tobacco, containing tobacco extract, spices and other food

grade additives. This standard was first laid down in 1999 and amended in 2003 and 2012. This revision is being

brought out to update its provisions in the light of developments in analytical methods, current industrial and

trade practices, and the prevailing statutory packaging and tobacco control regulations.









1 SCOPE

This standard prescribes the requirements, methods of test and sampling of Quiwam.

2 REFERENCES





IS No. Title












Doc. FAD 04(2729)C Draft Indian Standard Hookah tobacco, flake type Specification

(second revision of IS 4463)

2

Doc. FAD 04(2786)C Draft Indian Standard Tobacco and tobacco products Determination of reducing

and total sugars

3 DESCRIPTION

Quiwam is a paste type chewing tobacco preparation usually consumed along with betel leaf (see IS 10335). Air

cured tobacco of chewing variety is extracted with water and the extract is concentrated to a paste of required

consistency followed by mixing with aromatic spices, menthol, floral abstracts and essences, saffron, silver foil

and other permitted additives as required.

4 REQUIREMENTS

4.1 Silver Leaf

Silver leaf when used shall conform to IS 3110.

4.2 Additives

Any substances, if added, shall be of nature and purity which are suitable for use as food additives as permitted

under the Food Safety and Standards Act, 2006 and its rules and regulations.

4.3 The material shall also comply with the requirements given in Table 1.

Table 1 Requirements for Quiwam


Sl

No.


Ref to

(1) (2) (3) (4)



mass, Max

3.0 8 of IS 5643 or

IS 16026 or IS 16132

iii) Total sugar (on dry basis), percent by mass, Min 5.0 Doc: FAD 04(2786)

iv) Total ash (on dry basis), percent by mass, Max 25.0 10 of IS 5643

v) Silicated residues insoluble in hydrochloric acid (on


5.0 IS 16236

5 PACKING

The material shall be packed in glass or tin plate containers suitably lacquered from inside with food grade

lacquering material. The quantity per container and the type of container shall be as agreed to between the

purchaser and the vendor. The containers may be then packed in bulk container as agreed to between the

purchaser and the manufacturer.

6 MARKING

6 MARKING






d) Net quantity;



g) Statutory health warnings in the manner and in accordance with the provisions of the Rules framed

under the Cigarettes and Other Tobacco Products Act, 2003 (COTPA).

3






Standards.


Samples shall be drawn in accordance with the procedure given in Annex A or as agreed to between the

purchaser and the supplier. The conformity of the material in the lot to the requirements of this specification

shall be determined by testing in accordance with A-4 of Annex A.

8 TESTS

8.1 Tests shall be carried out as prescribed in 4, col 4 of Table1 and A-4 of Annex A.





ANNEX A

(Clauses 7 and 8.1)

SAMPLING OF QUIWAM



observed.



contamination.





the material.

A-1.5 Sampling shall be done by a person agreed to between the purchaser and vendor and in the presence of the

purchaser (or his representative) and the vendor (or his representative).


A-2.1 Lot

All the bulk containers of Quiwam in a single consignment of the material pertaining to the same brand shall



A-2.1.1 For ascertaining conformity of the materials in a lot to the requirements of this specification, tests shall

be carried out on each lot separately. The number of containers to be selected from the lot shall depend upon the

size of the lot and shall be in accordance with Table 2. These bulk containers shall be chosen at random from the

4

lot and for this purpose some random number table as agreed to between the purchaser and the vendor shall be

used (see IS 4905).


(Clause A-2.1.1)


(N) (n)

(1) (2)

Up to 15 5 3

16 and above 4

A-3 PREPARATION SAMPLES

On storage of quiwam, separation of the liquid and solid constituents may occur. It is necessary to mix the

contents of the container prior to drawing a sample and for this purpose the following procedure is

recommended.

A-3.0 Open the retail container at the edge of the lid or by uncapping or cutting as the case may be.

Reincorporate all the material adhering to the lid/cap/cut-out into the container. Mix the contents thoroughly by

stirring with a spoon or spatula in such a way that the top layers as well as contents of the lower layers are

stirred and mixed well.



sufficient so as to give about 150 g of the material. The material so taken out shall be mixed together; 50 g of

the mixed material shall be set aside for preparing composite sample (see A-3.2) and the balance will be divided

into three equal parts of about 30 g each. Each part shall constitute an individual sample representing the bulk

container and shall be transferred immediately to thoroughly clean and dry receptacles and sealed air-tight. The

receptacles shall be labelled with the particulars given under A-1.3.





3.2 Composite Sample


mixed together to form a composite sample of about 150 g for the lot.

A-3.2.2 The composite sample shall be divided into three equal parts. Each part shall constitute a composite

sample representing the lot and shall be transferred immediately to thoroughly clean and dry receptacles and

sealed air-tight. The receptacles shall be labelled with the particulars given under A-1.3 and marked one for the

purchaser, another for the vendor and the third for the referee. All the three samples shall bear the seals of the



Referee sample shall consist of a set of individual samples (see A-3.1) and composite sample (see A-3.2)

marked for this purpose, and shall bear the seals of the purchase and the supplier. These receptacles shall be kept

at a place agreed to between the purchaser and the vendor and shall be used in the case of a dispute between the

two.

5

A-4 TESTING PLAN


Tests for the determination of oven moisture and total nicotine alkaloids (Table 1) shall be conducted on each

of the individual samples in the set.

A-4.2 Composite Sample

Tests for the determination of the remaining characteristics in 4 and Table 1 shall be conducted in duplicate on

the composite sample.

A-5 CRITERIA FOR CONFORMITY







Draft for Comments Only Doc: No. FAD 04 (2809)C


CIGARETTES DETERMINATION OF LOSS OF TOBACCO FROM THE

ENDS METHOD USING A ROTATING CYLINDRICAL CAGE

(Adoption of ISO 3550-1 : 1997)

ICS No. 65.160

Not to be reproduced without the permission of

BIS or used as standard.

Last Date for Comments : April 20, 2015


NATIONAL FOREWORD

(Adoption clause to be added later)

This Indian Standard is identical with ISO 3550-1 : 1997 ‘Cigarettes Determination of loss of tobacco from the

ends Part 1 Method using a rotating cylindrical cage’ issued by the International Organization for

Standardization.

The text of ISO Standard has been approved as suitable for publication as an Indian Standard without deviations.

Certain conventions are however not identical to those used in Indian Standards. Attention is particularly drawn to

the following:

a) Wherever the words ‘International Standard’ appear referring to this standard, they should be read as

‘Indian Standard’.

b) Comma(,) has been used as a decimal marker while in Indian Standards, the current practice is to use a

point (.) as the decimal marker.

In this adopted standard, reference appears to certain International Standards for which Indian Standards also exist.

The corresponding Indian Standards, which are to be substituted in their respective places, are listed below along

with their degree of equivalence for the editions indicated:

International Standard Corresponding Indian Standard Degree of

Equivalence

ISO 2971, Cigarettes and filters rods

Determination of nominal diameter

Method using the laser beam measuring

device

IS 15795 : 2008/ ISO 2971 : 1998

Cigarette and filter rods Determination

of nominal diameter Method using laser

beam measuring apparatus

Identical

ISO 3402 : 1991, Tobacco and tobacco

products Atmosphere for conditioning

and testing

IS 16121 : 2013/ ISO 3402 : 1999

Tobacco and tobacco products

Atmosphere for conditioning and testing

Identical

ISO 6488, Tobacco Determination of

water content Karl Fischer method

IS 9379 : 2008/ISO 6488 : 2004 Tobacco

and tobacco products Determination of

water content Karl Fischer method

(third revision)

Identical

ISO 8243 : 1991, Cigarettes Sampling IS 12942 : 2008/ISO 8243 : 2006

Cigarettes Sampling (second revision)

Identical

In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or

calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ‘Rules for rounding off numerical

values (revised)’.

‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO 3550-1 : 1997’

For obtaining a hard copy of the complete document please contact/write to:

Scientist – F & Head

Food and Agriculture Department

Bureau of Indian Standards

Manak Bhavan

9 Bahadur Shah Zafar Marg

New Delhi – 110 002

Telefax: 011 23231128

Email: [email protected]



ROUTINE ANALYTICAL CIGARETTE-SMOKING MACHINE —

ADDITIONAL TEST METHODS FOR MACHINE VERIFICATION

(Adoption of ISO 7210 : 2013)

ICS No. 65.160





NATIONAL FOREWORD


This Indian Standard is identical with ISO 7210 : 2013 ‘Routine analytical cigarette-smoking machine — Additional

test methods for machine verification’ issued by the International Organization for Standardization.



the following:









Equivalence

ISO 3308 : 2012, Routine analytical

cigarette-smoking machine — Definitions

and standard conditions

IS 16022 : 2012/ISO 3308 : 2000 Routine

analytical cigarette - smoking machine

Definitions and standard conditions

Identical



and testing

IS 16121 : 2013/ ISO 3402 : 1999 Tobacco and

tobacco products Atmosphere for

conditioning and testing

Identical




‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO 7210 : 2013’





Manak Bhavan, 9 Bahadur Shah Zafar Marg


Telefax: 011 23231128; Email: [email protected]



CIGARETTES — DETERMINATION OF VENTILATION —

DEFINITIONS AND MEASUREMENT PRINCIPLES


ICS No. 65.160





NATIONAL FOREWORD


This Indian Standard is identical with ISO 9512 : 2002 ‘Cigarettes — Determination of ventilation — Definitions

and measurement principles’ issued by the International Organization for Standardization.



the following:









Equivalence

ISO 3308 : 2012, Routine analytical

cigarette-smoking machine — Definitions

and standard conditions

IS 16022 : 2012/ISO 3308 : 2000 Routine

analytical cigarette - smoking machine

Definitions and standard conditions

Identical



and testing

IS 16121 : 2013/ ISO 3402 : 1999 Tobacco and

tobacco products Atmosphere for

conditioning and testing

Identical

The technical committee responsible for the preparation of this standard may also review the following ISO

Standard and decide if this is acceptable for use in conjunction with this standard:

International Standard Title

ISO 6565 ,Tobacco and tobacco products — Draw resistance of cigarettes and pressure

drop of filter rods — Standard conditions and measurement






Manak Bhavan



Telefax: 011 23231128




CIGARETTES — DETERMINATION OF MENTHOL IN SMOKE

CONDENSATES — GAS CHROMATOGRAPHIC METHOD


ICS No. 65.160





NATIONAL FOREWORD


This Indian Standard is identical with ISO 13110 : 2012 ‘Cigarettes — Determination of menthol in smoke

condensates — Gas chromatographic method’ issued by the International Organization for Standardization.



the following:









Equivalence

ISO 4387, Cigarettes — Determination of

total and nicotine-free dry particulate

matter using a routine analytical smoking

machine

IS 16023 : 2012/ISO 4387 : 2000

Cigarettes Determination of total and

nicotine-free dry particulate matter using a

routine analytical smoking machine

Identical

ISO 8243 : 1991, Cigarettes Sampling IS 12942 : 2008/ISO 8243 : 2006

Cigarettes Sampling (second revision)

Identical









Manak Bhavan, 9 Bahadur Shah Zafar Marg

New Delhi – 110 002; Telefax: 011 23231128; Email: [email protected]



TOBACCO — DETERMINATION OF THE CONTENT OF REDUCING

CARBOHYDRATES — CONTINUOUS-FLOW ANALYSIS METHOD

(Adoption of ISO 15154 : 2003 alongwith Amd No. 1 to ISO 15154 : 2003 issued in May 2012)

ICS No. 65.160





NATIONAL FOREWORD


This Indian Standard is identical with ISO 15154 : 2003 ‘Tobacco — Determination of the content of reducing

carbohydrates — Continuous-flow analysis method’ issued by the International Organization for Standardization.

Amendment No. 1 to ISO 15154 : 2003 issued in May 2012 has also been incorporated in this standard.



the following:








‘FOR COMPLETE TEXT OF THE DOCUMENT, KINDLY REFER ISO 15154 : 2003 ALONGWITH

AMENDMENT NO. 1 TO ISO 15154 : 2003 ISSUED IN MAY 2012’





Manak Bhavan



Telefax: 011 23231128


Documents

Draft Indian Standard TOBACCO AND TOBACCO ...2786-2913)_18022015.pdf1 For BIS Use Only DRAFT FOR COMMENTS ONLY Doc: No. FAD 04(2786)C Draft Indian Standard TOBACCO AND TOBACCO PRODUCTS